US20210060451A1 - Plant and process for concentrating tartaric acid - Google Patents
Plant and process for concentrating tartaric acid Download PDFInfo
- Publication number
- US20210060451A1 US20210060451A1 US17/005,802 US202017005802A US2021060451A1 US 20210060451 A1 US20210060451 A1 US 20210060451A1 US 202017005802 A US202017005802 A US 202017005802A US 2021060451 A1 US2021060451 A1 US 2021060451A1
- Authority
- US
- United States
- Prior art keywords
- evaporation
- tartaric acid
- evaporation unit
- acid solution
- plant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/06—Flash distillation
- B01D3/065—Multiple-effect flash distillation (more than two traps)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/0082—Regulation; Control
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/14—Evaporating with heated gases or vapours or liquids in contact with the liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/26—Multiple-effect evaporating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/38—Steam distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0027—Condensation of vapours; Recovering volatile solvents by condensation by direct contact between vapours or gases and the cooling medium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0033—Other features
- B01D5/0048—Barometric condensation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
- C07C51/445—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation by steam distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
- B01D5/006—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
Definitions
- the present invention relates to a plant and process for concentrating tartaric acid, in particular by means of a continuous process.
- Tartaric acid is a white, crystalline diprotic organic acid. It is naturally present in many plants, especially grapes and tamarind (as well as other fruits).
- tartaric acid is produced in large amounts. It is obtained from lees, a by-product of wine fermentation.
- Tartaric acid has various fields of application.
- it can be added to foods as an antioxidant agent or to impart a sour taste. It is often added to certain foods such as candies, jams, and fruit juices to impart a sour taste thereto.
- It is used as an antioxidant and emulsifier in bread-making and in the preparation of leavening agents for cakes and bread. It is used in wine to balance the acidity thereof.
- tartaric acid has the ability to chelate metal ions such as calcium and magnesium. Therefore, it is used both in the agricultural industry and in the metallurgical industry, to favor, for example, the complexation of micronutrients present in soil or for cleaning metal surfaces (aluminum, copper, iron, or metal alloys).
- the production process of tartaric acid includes a concentration step in which the diluted tartaric acid undergoes a concentration process, in order to obtain concentrated tartaric acid.
- This process usually takes place inside an evaporation plant.
- the physical principle on which this type of plant is based is an evaporation principle which exploits the different boiling points (and therefore evaporation) of the components of a solution (diluted tartaric acid in this case).
- the solutions subjected to this type of process usually consist of a solute having a higher boiling point than that of the solvent. Thereby, by heating the solution up to the solvent boiling temperature, the latter will evaporate, concentrating the solution.
- the tartaric acid solutions to be concentrated are usually solutions whose tendency to crystallization is high, which makes them problematic solutions when placed in an evaporation plant.
- using an easy crystallization solution inside an evaporation plant can cause the formation of encrustations inside the walls of the plant where the solution flows, with consequent damage to the plant itself.
- FIG. 1 shows the plant for concentrating tartaric acid according to the present invention.
- FIG. 2 shows a detail of the plant of FIG. 1 .
- a plant 10 for concentrating a tartaric acid solution comprising:
- the tartaric acid solution comprises tartaric acid and sulfuric acid, the latter at a concentration between 3% and 5%, preferably about 4%.
- each of said first 12 and second 14 evaporation units comprises:
- a heat-exchange evaporation chamber 22 in which the first vapor comes into contact with the tartaric acid solution to be concentrated
- a liquid-aeriform separation chamber 24 connected to a head portion 26 of said evaporation chamber 22 .
- the first vapor is saturated aqueous vapor having a temperature between 70° C. and 90° C., preferably about 80° C.
- said heat exchange evaporation chamber 22 is an apparatus known to those skilled in the art in which thermal energy is exchanged between two elements having different temperatures.
- the above elements are the tartaric acid solution and the first vapor.
- the heat-exchange evaporation chamber 22 receives the first low-temperature vapor, by means of which the exchange of thermal energy takes place between the first vapor and the tartaric acid solution.
- This thermal energy exchange allows to heat the solution until the boiling temperature of the tartaric acid solution is reached, resulting in the formation of a second vapor (vapor of the solvent contained in the tartaric acid solution) and accumulation in the head portion 26 of the evaporation chamber 22 of an aeriform phase consisting of the aforesaid second vapor. Indeed, the amount of energy required for evaporation is supplied by the first low-temperature vapor.
- the heat-exchange evaporation chamber 22 of the first evaporation unit 12 receives the first low-temperature vapor from the system for feeding the first low-temperature vapor 20 .
- the liquid-aeriform separation chamber 24 is also preferably an apparatus known to those skilled in the art in which a separation of the aeriform phase coming from the head portion 26 of the evaporation chamber 22 is carried out.
- the aforesaid aeriform phase may also comprise, in addition to the second vapor produced by the evaporation of the tartaric acid solution, the tartaric acid particles dragged from the evaporation chamber 22 . Therefore, inside the liquid-aeriform separation chamber 24 , there is a separation between the properly said aeriform phase (second vapor) and the dragged tartaric acid particles.
- the tartaric acid solution has a temperature between 50° C. and 60° C., preferably about 56° C., and a pressure between 0.07 BarA and 0.11 BarA, preferably about 0.09 BarA.
- the tartaric acid solution has a temperature between 60° C. and 70° C., preferably about 66° C.
- the barometric condenser 18 is connected to a vacuum pump 52 and to a system for circulating water 54 inside the condenser.
- the barometric condenser 18 condenses the properly said aeriform phase exiting the second evaporation unit 14 .
- the separation chamber 24 of the second evaporation unit 14 is connected to the barometric condenser 18 through an acidic solution separation chamber 44 being placed in an intermediate position between the separation chamber 24 of the second evaporation unit 14 and the barometric condenser 18 .
- the function of the acidic solution separation chamber 44 is to separate any acidic residues present in the properly said aeriform phase exiting the separation chamber 24 of the second evaporation unit 14 .
- Each of said first 12 and second 14 evaporation units also preferably comprises a connecting portion 28 which connects the liquid-aeriform separation chamber 24 to a bottom portion 30 of said evaporation chamber 22 , in which said connecting portion 28 comprises a column 32 which extends along a vertical axis.
- the column 32 of the first evaporation unit 12 is connected to the pump for feeding a diluted tartaric acid solution 16 , thus allowing the introduction of the diluted tartaric acid solution to be concentrated into the first evaporation unit 12 and therefore into the plant 10 .
- Each of said first 12 and second 14 evaporation units further comprises, preferably, a recirculation pump for the tartaric acid solution operatively connected to said connecting portion 28 , for recirculating the tartaric acid solution from said separation chamber 24 to said evaporation chamber 22 .
- the tartaric acid particles dragged from the evaporation chamber 22 and separated from the properly said aeriform phase inside the liquid-aeriform separation chamber 24 , fall by gravity into the column 32 , joining the tartaric acid solution already present in the connecting portion 28 .
- the presence of the recirculation pump 34 allowing the recirculation of the tartaric acid solution, advantageously allows to have a forced-circulation plant 10 for concentrating a tartaric acid solution.
- the forced circulation creates a turbulent motion inside the tartaric acid solution which ensures a high exchange coefficient between the first vapor and the tartaric acid solution and allows an easy concentration of a solution tending to crystallization such as that used in the plant 10 according to the present invention.
- recirculation pumps 34 and of a pair of evaporation units placed in series advantageously ensures low energy consumption.
- said first 12 and second 14 evaporation units are, preferably, connected by a pipe for transferring the partially concentrated tartaric acid solution 36 placed at a bottom portion 38 of said evaporation units 12 ; 14 and by a pipe for transferring the properly said aeriform phase 40 from a head portion 42 of the separation chamber 24 of the first evaporation unit 12 to the evaporation chamber 22 of the second evaporation unit 14 .
- connections not only allow the series connection of the two evaporation units 12 ; 14 , but also the passage of the partially-concentrated tartaric acid solution and of the properly said aeriform phase, created in the first evaporation unit 12 , from the first evaporation unit 12 to the second evaporation unit 14 .
- the pipe for transferring the partially concentrated solution 36 preferably connects a bottom portion of the connecting portion 28 of the first evaporation unit 12 , placed downstream of the column 32 , with a bottom portion of the column 32 of the second evaporation unit 14 .
- the column of the connecting portion 28 of the second evaporation unit 14 preferably and advantageously comprises a pair of facing-flange pressure sensors 46 , each coupled to a fluid separator preferably in tantalum, in which the pressure sensors 46 are placed at a distance between 1.5 m and 2.5 m, preferably about m, and are connected to a differential pressure transmitter 48 in turn connected to a volumetric pump 50 for extracting concentrated tartaric acid from the plant 10 , said volumetric pump 50 being controlled on the basis of an electrical signal sent by the differential pressure transmitter 48 between 4 mA and 20 mA.
- said control takes place by means of a feedback control adapted to allow the extraction of concentrated tartaric acid from the plant 10 only when the pressure value detected by the differential pressure transmitter 48 is within ideal values between kg/l and 1.5 kg/l, values which correspond to the sending, by the differential pressure transmitter 48 , of the electrical signal between 4 mA and 20 mA.
- the pair of sensors 46 is preferably placed at the aforesaid distance along a vertical axis along which the column 32 of the connecting portion 28 extends.
- the fluid separators are used when the pressure sensors 46 to which they are coupled must not come into contact with the process fluid. Therefore, they serve the function of transmitting the pressure variations of the fluid flowing in the plant 10 to the instrument (the differential pressure transmitter 48 , in the case of the present invention), while keeping it isolated from the pressure sensor 46 .
- Suitable types of fluid separators according to the present invention are, for example, fluid separators in titanium, nickel, tantalum.
- the fluid separators of the present invention are preferably in tantalum.
- the differential pressure transmitter 48 is also preferably connected to a flow rate sensor 56 placed downstream of the volumetric pump 50 .
- the function of the flow rate sensor 56 is to measure the flow rate of concentrated tartaric acid exiting the plant 10 .
- the flow rate sensor 56 carries out a second control on the volumetric pump 50 .
- said second control also takes place by means of a feedback control adapted to keep the flow rate within ideal values.
- said ideal values are between 0 m 3 /h and 10 m 3 /h.
- the present invention further relates to a process for concentrating tartaric acid comprising the steps of:
- the process for concentrating tartaric acid preferably comprises the following steps:
- the process for concentrating tartaric acid preferably begins with the introduction, by means of the feed pump 16 , of the diluted tartaric acid solution into the column 32 of the connecting portion 28 of the first evaporation unit 12 .
- the diluted tartaric acid solution flows, due to the recirculation pump 34 , into the heat-exchange evaporation chamber 22 of the first evaporation unit 12 .
- the diluted tartaric acid solution encounters the first low-temperature vapor, coming from the feed system 20 , and an exchange of thermal energy takes place between the first vapor and the diluted tartaric acid solution. This exchange of thermal energy leads to an increase in the temperature of the diluted tartaric acid solution until the boiling temperature thereof is reached.
- the solvent contained within the solution begins to evaporate, creating a second vapor.
- An aeriform phase thus accumulates in the head portion 26 of the evaporation chamber 22 , consisting of the aforesaid second vapor and any residual tartaric acid particles which are dragged during the evaporation.
- This aeriform phase then passes inside the liquid-aeriform separation chamber 24 of the first evaporation unit 12 , in which the separation takes place between the properly said aeriform phase (second vapor) and the tartaric acid particles dragged by the head portion 26 of the evaporation chamber 22 .
- the properly said aeriform phase passes instead inside the pipe for transferring the properly said aeriform phase 40 to enter the heat-exchange evaporation chamber 22 of the second evaporation unit 14 where it meets the partially concentrated tartaric acid solution coming from the first evaporation unit 12 .
- the pipe for transferring the partially concentrated tartaric acid solution 36 which connects to a bottom portion of the column 32 extends from a bottom portion of the connecting portion 28 , placed downstream of the column 32 , of the first evaporation unit 12 of the connecting portion 28 of the second evaporation unit 14 .
- the partially concentrated tartaric acid solution passes from the first evaporation unit 12 to the second evaporation unit 14 and enters the column 32 of the connecting portion 28 of the second evaporation unit 14 .
- the partially concentrated tartaric acid solution is transported here, due to the action of the recirculation pump 34 , inside the heat-exchange evaporation chamber 22 of the second evaporation unit 14 where it meets the aforesaid properly said aeriform phase and where a heat exchange between the two takes place.
- the properly said aeriform phase heats the partially concentrated tartaric acid solution until it reaches the boiling temperature thereof. Once this temperature has been reached, the solvent of the partially concentrated solution begins to evaporate, creating, as for the first evaporation unit 12 , an aeriform phase comprising a second vapor and any tartaric acid particles.
- the aeriform phase passes into the separation chamber 24 (of the second evaporation unit 14 ) where the separation between the properly said aeriform phase (second vapor) and the tartaric acid particles takes place, which fall by gravity into the column 32 of the connecting portion 28 of the second evaporation unit 14 .
- the properly said aeriform phase of the second evaporation unit 14 instead passes inside the acidic solution separation chamber 44 where the separation of any acidic gases present in the properly said aeriform phase takes place.
- the properly said aeriform phase exiting the acidic solution separation chamber 44 passes inside the barometric condenser 18 where the condensable vapors are condensed and extracted from the plant 10 , while any non-condensable gases are extracted by means of a vacuum pump 52 .
- the pair of pressure sensors 46 is present inside the column 32 of the connecting portion 28 of the second evaporation unit 14 , the pair measuring the pressure of the tartaric acid solution in transit.
- the pressure measurement value is sent to the differential pressure transmitter 48 which when it detects a pressure value between 1 kg/l and 1.5 kg/l (preferably when it detects a pressure signal of about 1.3 kg/l), pressure values set as ideal set points, sends a signal (between 4 mA and 20 mA, preferably about 17 mA) to the volumetric pump 50 , thus controlling the extraction of the concentrated tartaric acid solution from the second evaporation unit 14 .
- a flow rate sensor 56 Downstream of the volumetric pump 50 there is also preferably a flow rate sensor 56 , the purpose of which is to measure the flow rate of the concentrated tartaric acid solution exiting the second evaporation unit 14 . If the measured range is between 0 m 3 /h and 10 m 3 /h, (preferably about 4.5 m 3 /h), flow rates set as ideal set points, the flow rate sensor 56 sends a second feedback control signal to the volumetric pump 50 , controlling the extraction activity of concentrated tartaric acid from the plant 10 .
- the plant 10 and the process for concentrating tartaric acid according to the present invention have the advantages of ensuring low energy consumption, allowing an easy concentration of solutions tending to crystallization, and allowing the continuous measurement of the tartaric acid concentration to be concentrated.
- the plant 10 and the process for concentrating tartaric acid according to the present invention also have the advantage of accurately obtaining concentrated tartaric acid, due to the repeatability provided by the double feedback control mechanism provided in the plant 10 and in the related process.
- the presence of the two feedback controls allows to maintain the pressure values, and therefore the concentration, of the concentrated tartaric acid and the values of the flow rate of concentrated tartaric acid leaving the plant 10 around ideal pre-set values, thus ensuring accuracy and repeatability.
Abstract
Description
- The present invention relates to a plant and process for concentrating tartaric acid, in particular by means of a continuous process.
- Tartaric acid is a white, crystalline diprotic organic acid. It is naturally present in many plants, especially grapes and tamarind (as well as other fruits). One of the salts thereof, potassium bitartrate, commonly known as cream of tartar, develops naturally in the winemaking process.
- Industrially, tartaric acid is produced in large amounts. It is obtained from lees, a by-product of wine fermentation.
- Tartaric acid has various fields of application. One of the uses thereof, when mixed with sodium bicarbonate, is as a leavening agent. As such, it can be added to foods as an antioxidant agent or to impart a sour taste. It is often added to certain foods such as candies, jams, and fruit juices to impart a sour taste thereto. It is used as an antioxidant and emulsifier in bread-making and in the preparation of leavening agents for cakes and bread. It is used in wine to balance the acidity thereof. It is used in the preparation of medicines: for example, mixed with sodium bicarbonate, it is used in the preparation of effervescent products to aid digestion. As for industrial applications, tartaric acid has the ability to chelate metal ions such as calcium and magnesium. Therefore, it is used both in the agricultural industry and in the metallurgical industry, to favor, for example, the complexation of micronutrients present in soil or for cleaning metal surfaces (aluminum, copper, iron, or metal alloys).
- To date, the production process of tartaric acid includes a concentration step in which the diluted tartaric acid undergoes a concentration process, in order to obtain concentrated tartaric acid.
- This process usually takes place inside an evaporation plant. The physical principle on which this type of plant is based is an evaporation principle which exploits the different boiling points (and therefore evaporation) of the components of a solution (diluted tartaric acid in this case). Indeed, the solutions subjected to this type of process usually consist of a solute having a higher boiling point than that of the solvent. Thereby, by heating the solution up to the solvent boiling temperature, the latter will evaporate, concentrating the solution.
- The possibility of arranging a plant capable of concentrating tartaric acid which is produced efficiently and with low energy consumption is thus a need felt in the market.
- Furthermore, the tartaric acid solutions to be concentrated are usually solutions whose tendency to crystallization is high, which makes them problematic solutions when placed in an evaporation plant. Indeed, using an easy crystallization solution inside an evaporation plant can cause the formation of encrustations inside the walls of the plant where the solution flows, with consequent damage to the plant itself.
- When working with an evaporation plant for concentrating solutions, another parameter to consider is the measurement of the concentration of the solution to be concentrated. In fact, it is important that the solution is only extracted from the plant when it is certain that the solution has reached a certain concentration value. Therefore, the identification and use, within the plant, of a system which allows the continuous measurement of the concentration of the solution to be concentrated is an important aspect for the good yield of the concentration process.
- Therefore, it is object of the present invention to provide a plant and process for concentrating tartaric acid which is efficient, ensures low energy consumption, allows an easy concentration of solutions tending to crystallization, and has a system for the continuous measurement of the tartaric acid concentration to be concentrated.
- This object is achieved by a plant and process for concentrating tartaric acid as outlined in the appended claims, the definitions of which form an integral part of the present patent application.
- The invention will be better understood from the following detailed description of preferred embodiments thereof, given by way of not limiting example, with reference to the accompanying drawings, in which:
-
FIG. 1 shows the plant for concentrating tartaric acid according to the present invention. -
FIG. 2 shows a detail of the plant ofFIG. 1 . - In the accompanying drawings, equal or similar elements will be indicated by the same reference numerals.
- With reference to
FIGS. 1 and 2 , a first object of the present invention is shown, i.e., aplant 10 for concentrating a tartaric acid solution comprising: -
- a first 12 and a second 14 evaporation unit, in which said first 12 and second 14 evaporation units are arranged in series;
- a pump for feeding a diluted
tartaric acid solution 16 into saidfirst evaporation unit 12; - a
barometric condenser 18 placed downstream of saidsecond evaporation unit 14, - a system for feeding a first low-
temperature vapor 20 into saidfirst evaporation unit 12.
- Preferably, the tartaric acid solution comprises tartaric acid and sulfuric acid, the latter at a concentration between 3% and 5%, preferably about 4%.
- Preferably, each of said first 12 and second 14 evaporation units comprises:
- i) a heat-
exchange evaporation chamber 22, in which the first vapor comes into contact with the tartaric acid solution to be concentrated,
ii) a liquid-aeriform separation chamber 24, connected to ahead portion 26 of saidevaporation chamber 22. - Preferably, the first vapor is saturated aqueous vapor having a temperature between 70° C. and 90° C., preferably about 80° C.
- Preferably, said heat
exchange evaporation chamber 22 is an apparatus known to those skilled in the art in which thermal energy is exchanged between two elements having different temperatures. According to a preferred embodiment of the present invention, the above elements are the tartaric acid solution and the first vapor. In fact, the heat-exchange evaporation chamber 22 receives the first low-temperature vapor, by means of which the exchange of thermal energy takes place between the first vapor and the tartaric acid solution. This thermal energy exchange allows to heat the solution until the boiling temperature of the tartaric acid solution is reached, resulting in the formation of a second vapor (vapor of the solvent contained in the tartaric acid solution) and accumulation in thehead portion 26 of theevaporation chamber 22 of an aeriform phase consisting of the aforesaid second vapor. Indeed, the amount of energy required for evaporation is supplied by the first low-temperature vapor. - Preferably the heat-
exchange evaporation chamber 22 of thefirst evaporation unit 12 receives the first low-temperature vapor from the system for feeding the first low-temperature vapor 20. - The liquid-
aeriform separation chamber 24 is also preferably an apparatus known to those skilled in the art in which a separation of the aeriform phase coming from thehead portion 26 of theevaporation chamber 22 is carried out. In fact, the aforesaid aeriform phase may also comprise, in addition to the second vapor produced by the evaporation of the tartaric acid solution, the tartaric acid particles dragged from theevaporation chamber 22. Therefore, inside the liquid-aeriform separation chamber 24, there is a separation between the properly said aeriform phase (second vapor) and the dragged tartaric acid particles. - Two unitary operations are thus carried out inside the
evaporation chamber 22 and the separation chamber 24: the heat exchange between the first vapor and the tartaric acid solution and the separation between the properly said aeriform phase and the dragged tartaric acid particles. - Preferably inside the heat-
exchange evaporation chamber 22 of thesecond evaporation unit 14, the tartaric acid solution has a temperature between 50° C. and 60° C., preferably about 56° C., and a pressure between 0.07 BarA and 0.11 BarA, preferably about 0.09 BarA. While on the other hand, preferably, inside the heat-exchange evaporation chamber 22 of thefirst evaporation unit 12, the tartaric acid solution has a temperature between 60° C. and 70° C., preferably about 66° C. - According to a preferred embodiment of the invention, the
barometric condenser 18 is connected to avacuum pump 52 and to a system for circulatingwater 54 inside the condenser. Advantageously, thebarometric condenser 18 condenses the properly said aeriform phase exiting thesecond evaporation unit 14. - Furthermore, preferably, the
separation chamber 24 of thesecond evaporation unit 14 is connected to thebarometric condenser 18 through an acidicsolution separation chamber 44 being placed in an intermediate position between theseparation chamber 24 of thesecond evaporation unit 14 and thebarometric condenser 18. The function of the acidicsolution separation chamber 44 is to separate any acidic residues present in the properly said aeriform phase exiting theseparation chamber 24 of thesecond evaporation unit 14. - Each of said first 12 and second 14 evaporation units also preferably comprises a connecting
portion 28 which connects the liquid-aeriform separation chamber 24 to abottom portion 30 of saidevaporation chamber 22, in which said connectingportion 28 comprises acolumn 32 which extends along a vertical axis. - Preferably, the
column 32 of thefirst evaporation unit 12 is connected to the pump for feeding a dilutedtartaric acid solution 16, thus allowing the introduction of the diluted tartaric acid solution to be concentrated into thefirst evaporation unit 12 and therefore into theplant 10. - Each of said first 12 and second 14 evaporation units further comprises, preferably, a recirculation pump for the tartaric acid solution operatively connected to said connecting
portion 28, for recirculating the tartaric acid solution from saidseparation chamber 24 to saidevaporation chamber 22. - According to a preferred embodiment, the tartaric acid particles, dragged from the
evaporation chamber 22 and separated from the properly said aeriform phase inside the liquid-aeriform separation chamber 24, fall by gravity into thecolumn 32, joining the tartaric acid solution already present in the connectingportion 28. The presence of therecirculation pump 34, allowing the recirculation of the tartaric acid solution, advantageously allows to have a forced-circulation plant 10 for concentrating a tartaric acid solution. The forced circulation creates a turbulent motion inside the tartaric acid solution which ensures a high exchange coefficient between the first vapor and the tartaric acid solution and allows an easy concentration of a solution tending to crystallization such as that used in theplant 10 according to the present invention. - Furthermore, the presence of recirculation pumps 34 and of a pair of evaporation units placed in series advantageously ensures low energy consumption.
- According to a preferred embodiment of the
plant 10 of the present invention, said first 12 and second 14 evaporation units are, preferably, connected by a pipe for transferring the partially concentratedtartaric acid solution 36 placed at abottom portion 38 of saidevaporation units 12; 14 and by a pipe for transferring the properly saidaeriform phase 40 from ahead portion 42 of theseparation chamber 24 of thefirst evaporation unit 12 to theevaporation chamber 22 of thesecond evaporation unit 14. - These connections not only allow the series connection of the two
evaporation units 12; 14, but also the passage of the partially-concentrated tartaric acid solution and of the properly said aeriform phase, created in thefirst evaporation unit 12, from thefirst evaporation unit 12 to thesecond evaporation unit 14. In particular, the pipe for transferring the partiallyconcentrated solution 36 preferably connects a bottom portion of the connectingportion 28 of thefirst evaporation unit 12, placed downstream of thecolumn 32, with a bottom portion of thecolumn 32 of thesecond evaporation unit 14. - Still according to a preferred embodiment of the
plant 10 according to the present invention, the column of the connectingportion 28 of thesecond evaporation unit 14 preferably and advantageously comprises a pair of facing-flange pressure sensors 46, each coupled to a fluid separator preferably in tantalum, in which thepressure sensors 46 are placed at a distance between 1.5 m and 2.5 m, preferably about m, and are connected to adifferential pressure transmitter 48 in turn connected to avolumetric pump 50 for extracting concentrated tartaric acid from theplant 10, saidvolumetric pump 50 being controlled on the basis of an electrical signal sent by thedifferential pressure transmitter 48 between 4 mA and 20 mA. - Preferably, said control takes place by means of a feedback control adapted to allow the extraction of concentrated tartaric acid from the
plant 10 only when the pressure value detected by thedifferential pressure transmitter 48 is within ideal values between kg/l and 1.5 kg/l, values which correspond to the sending, by thedifferential pressure transmitter 48, of the electrical signal between 4 mA and 20 mA. - The pair of
sensors 46 is preferably placed at the aforesaid distance along a vertical axis along which thecolumn 32 of the connectingportion 28 extends. - As known, the fluid separators are used when the
pressure sensors 46 to which they are coupled must not come into contact with the process fluid. Therefore, they serve the function of transmitting the pressure variations of the fluid flowing in theplant 10 to the instrument (thedifferential pressure transmitter 48, in the case of the present invention), while keeping it isolated from thepressure sensor 46. Suitable types of fluid separators according to the present invention are, for example, fluid separators in titanium, nickel, tantalum. The fluid separators of the present invention are preferably in tantalum. - The
differential pressure transmitter 48 is also preferably connected to aflow rate sensor 56 placed downstream of thevolumetric pump 50. The function of theflow rate sensor 56 is to measure the flow rate of concentrated tartaric acid exiting theplant 10. Preferably, theflow rate sensor 56 carries out a second control on thevolumetric pump 50. Preferably said second control also takes place by means of a feedback control adapted to keep the flow rate within ideal values. Preferably said ideal values are between 0 m3/h and 10 m3/h. - For a detailed description of the operation and diagram of the signals transmitted by the
pressure sensors 46, and by the flow rate sensors, to thevolumetric pump 50, reference should be made to the following of the present description. - The present invention further relates to a process for concentrating tartaric acid comprising the steps of:
-
- providing a
plant 10 according to the above description; - performing a first concentration, by evaporation, of the diluted tartaric acid solution, inside the
first evaporation unit 12; - performing a second concentration, by evaporation, of the partially concentrated tartaric acid solution from the
first evaporation unit 12, inside thesecond evaporation unit 14;
- providing a
- According to a preferred embodiment of the present invention, the process for concentrating tartaric acid preferably comprises the following steps:
-
- providing a
plant 10 according to the above description; - performing a first concentration, by evaporation, of the diluted tartaric acid solution, inside the
first evaporation unit 12; - performing a second concentration, by evaporation, of the partially concentrated tartaric acid solution from the
first evaporation unit 12, inside thesecond evaporation unit 14; - setting, as a basal pressure difference ΔP measured between the first and second sensors of the pair of
sensors 46 present in thecolumn 32 of the connectingportion 28 of thesecond evaporation unit 14, the pressure difference which would be measured in a 2 m high water column, corresponding to a density of 1 kg/l, and assigning the zero value to said ΔP. - measuring the pressure of the tartaric acid solution flowing inside the
column 32 of the connectingportion 28 of thesecond evaporation unit 14 by means of the aforesaid pair ofpressure sensors 46; - sending the measured pressure values to the
differential pressure transmitter 48, which, when detecting a ΔP value equal to a density between 1 kg/l and 1.5 kg/l, preferably about 1.3 kg/l, sends an electrical feedback control signal between 4 mA and 20 mA, preferably about 17 mA, to thevolumetric pump 50 which controls the extraction of the concentrated tartaric acid solution from thesecond evaporation unit 14.
- providing a
- Therefore, the process for concentrating tartaric acid according to the present invention preferably begins with the introduction, by means of the
feed pump 16, of the diluted tartaric acid solution into thecolumn 32 of the connectingportion 28 of thefirst evaporation unit 12. From here the diluted tartaric acid solution flows, due to therecirculation pump 34, into the heat-exchange evaporation chamber 22 of thefirst evaporation unit 12. Here the diluted tartaric acid solution encounters the first low-temperature vapor, coming from thefeed system 20, and an exchange of thermal energy takes place between the first vapor and the diluted tartaric acid solution. This exchange of thermal energy leads to an increase in the temperature of the diluted tartaric acid solution until the boiling temperature thereof is reached. Once the aforesaid boiling temperature has been reached, the solvent contained within the solution begins to evaporate, creating a second vapor. An aeriform phase thus accumulates in thehead portion 26 of theevaporation chamber 22, consisting of the aforesaid second vapor and any residual tartaric acid particles which are dragged during the evaporation. This aeriform phase then passes inside the liquid-aeriform separation chamber 24 of thefirst evaporation unit 12, in which the separation takes place between the properly said aeriform phase (second vapor) and the tartaric acid particles dragged by thehead portion 26 of theevaporation chamber 22. The tartaric acid particles dragged by thehead portion 26 of theevaporation chamber 22 fall by gravity into thecolumn 32 of the connectingportion 28 of thefirst evaporation unit 12, thus adding themselves to the diluted tartaric acid solution coming from thefeed pump 16. The properly said aeriform phase passes instead inside the pipe for transferring the properly saidaeriform phase 40 to enter the heat-exchange evaporation chamber 22 of thesecond evaporation unit 14 where it meets the partially concentrated tartaric acid solution coming from thefirst evaporation unit 12. In fact, the pipe for transferring the partially concentratedtartaric acid solution 36 which connects to a bottom portion of thecolumn 32 extends from a bottom portion of the connectingportion 28, placed downstream of thecolumn 32, of thefirst evaporation unit 12 of the connectingportion 28 of thesecond evaporation unit 14. Through thispipe 36 the partially concentrated tartaric acid solution passes from thefirst evaporation unit 12 to thesecond evaporation unit 14 and enters thecolumn 32 of the connectingportion 28 of thesecond evaporation unit 14. The partially concentrated tartaric acid solution is transported here, due to the action of therecirculation pump 34, inside the heat-exchange evaporation chamber 22 of thesecond evaporation unit 14 where it meets the aforesaid properly said aeriform phase and where a heat exchange between the two takes place. The properly said aeriform phase heats the partially concentrated tartaric acid solution until it reaches the boiling temperature thereof. Once this temperature has been reached, the solvent of the partially concentrated solution begins to evaporate, creating, as for thefirst evaporation unit 12, an aeriform phase comprising a second vapor and any tartaric acid particles. As in thefirst evaporation unit 12, also in thesecond evaporation unit 14 the aeriform phase passes into the separation chamber 24 (of the second evaporation unit 14) where the separation between the properly said aeriform phase (second vapor) and the tartaric acid particles takes place, which fall by gravity into thecolumn 32 of the connectingportion 28 of thesecond evaporation unit 14. The properly said aeriform phase of thesecond evaporation unit 14 instead passes inside the acidicsolution separation chamber 44 where the separation of any acidic gases present in the properly said aeriform phase takes place. The properly said aeriform phase exiting the acidicsolution separation chamber 44 passes inside thebarometric condenser 18 where the condensable vapors are condensed and extracted from theplant 10, while any non-condensable gases are extracted by means of avacuum pump 52. - The pair of
pressure sensors 46 is present inside thecolumn 32 of the connectingportion 28 of thesecond evaporation unit 14, the pair measuring the pressure of the tartaric acid solution in transit. The pressure measurement value is sent to thedifferential pressure transmitter 48 which when it detects a pressure value between 1 kg/l and 1.5 kg/l (preferably when it detects a pressure signal of about 1.3 kg/l), pressure values set as ideal set points, sends a signal (between 4 mA and 20 mA, preferably about 17 mA) to thevolumetric pump 50, thus controlling the extraction of the concentrated tartaric acid solution from thesecond evaporation unit 14. - Downstream of the
volumetric pump 50 there is also preferably aflow rate sensor 56, the purpose of which is to measure the flow rate of the concentrated tartaric acid solution exiting thesecond evaporation unit 14. If the measured range is between 0 m3/h and 10 m3/h, (preferably about 4.5 m3/h), flow rates set as ideal set points, theflow rate sensor 56 sends a second feedback control signal to thevolumetric pump 50, controlling the extraction activity of concentrated tartaric acid from theplant 10. - Therefore, the
plant 10 and the process for concentrating tartaric acid according to the present invention have the advantages of ensuring low energy consumption, allowing an easy concentration of solutions tending to crystallization, and allowing the continuous measurement of the tartaric acid concentration to be concentrated. - The
plant 10 and the process for concentrating tartaric acid according to the present invention also have the advantage of accurately obtaining concentrated tartaric acid, due to the repeatability provided by the double feedback control mechanism provided in theplant 10 and in the related process. The presence of the two feedback controls allows to maintain the pressure values, and therefore the concentration, of the concentrated tartaric acid and the values of the flow rate of concentrated tartaric acid leaving theplant 10 around ideal pre-set values, thus ensuring accuracy and repeatability.
Claims (9)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
IT102019000015291 | 2019-08-30 | ||
IT102019000015291A IT201900015291A1 (en) | 2019-08-30 | 2019-08-30 | PLANT AND PROCESS FOR THE CONCENTRATION OF TARTARIC ACID |
Publications (2)
Publication Number | Publication Date |
---|---|
US20210060451A1 true US20210060451A1 (en) | 2021-03-04 |
US11752446B2 US11752446B2 (en) | 2023-09-12 |
Family
ID=69468962
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US17/005,802 Active US11752446B2 (en) | 2019-08-30 | 2020-08-28 | Plant and process for concentrating tartaric acid |
Country Status (5)
Country | Link |
---|---|
US (1) | US11752446B2 (en) |
EP (1) | EP3785782B1 (en) |
AU (1) | AU2020223741A1 (en) |
ES (1) | ES2937970T3 (en) |
IT (1) | IT201900015291A1 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114887340A (en) * | 2022-04-29 | 2022-08-12 | 江苏才信通科技有限公司 | Double-effect MVR forced countercurrent circulation falling film evaporation crystallization system |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2367215A (en) * | 1940-11-01 | 1945-01-16 | Buffalo Foundry & Machine Co | Differential pressure responsive device |
US4046010A (en) * | 1976-11-12 | 1977-09-06 | Beckman Instruments, Inc. | Pressure transducer with welded tantalum diaphragm |
US11377414B2 (en) * | 2019-08-30 | 2022-07-05 | Distillerie Mazzari S.P.A | Plant and process for concentrating tartaric acid |
Family Cites Families (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1513305A (en) * | 1919-10-31 | 1924-10-28 | Barbet Emile Augustin | Process and apparatus for concentrating grape juices |
US1831121A (en) * | 1930-01-23 | 1931-11-10 | Buffalo Foundry & Machine Comp | Evaporating apparatus |
US2184579A (en) * | 1936-06-24 | 1939-12-26 | American Lurgi Corp | Distillation of mixtures of high boiling point liquids |
US2510233A (en) * | 1944-03-06 | 1950-06-06 | Blaw Knox Co | Apparatus for evaporating viscous liquids |
US2524753A (en) * | 1946-01-10 | 1950-10-10 | Joseph L Betts | Method of recovering heat and suspended chemical particles from gases resulting fromthe combustion of a pulp residual liquor and apparatus therefor |
US2838108A (en) * | 1949-08-03 | 1958-06-10 | Sumiya Shinzo | Multiple effect vacuum evaporator |
US3289736A (en) * | 1964-06-30 | 1966-12-06 | Rosenblad Corp | Temperature control for evaporation system |
US3855079A (en) * | 1972-12-26 | 1974-12-17 | Hanover Res Corp | Process and apparatus for recovering residual oil from solids dehydrated in an oil medium and grossly deoiled |
CH558760A (en) * | 1973-05-14 | 1975-02-14 | Bertrams Ag Hch | PROCESS AND EQUIPMENT FOR REMOVING CONTAMINATION FROM A LIQUID. |
FR2975479B1 (en) * | 2011-05-16 | 2019-07-12 | Montpellier Engineering | DEVICE FOR EVAPORATION / CONDENSATION |
DE102016214019A1 (en) * | 2016-07-29 | 2018-02-01 | Siemens Aktiengesellschaft | Device for separating product water from contaminated raw water and method for operating this device |
-
2019
- 2019-08-30 IT IT102019000015291A patent/IT201900015291A1/en unknown
-
2020
- 2020-08-26 ES ES20192802T patent/ES2937970T3/en active Active
- 2020-08-26 EP EP20192802.5A patent/EP3785782B1/en active Active
- 2020-08-27 AU AU2020223741A patent/AU2020223741A1/en active Pending
- 2020-08-28 US US17/005,802 patent/US11752446B2/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2367215A (en) * | 1940-11-01 | 1945-01-16 | Buffalo Foundry & Machine Co | Differential pressure responsive device |
US4046010A (en) * | 1976-11-12 | 1977-09-06 | Beckman Instruments, Inc. | Pressure transducer with welded tantalum diaphragm |
US11377414B2 (en) * | 2019-08-30 | 2022-07-05 | Distillerie Mazzari S.P.A | Plant and process for concentrating tartaric acid |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114887340A (en) * | 2022-04-29 | 2022-08-12 | 江苏才信通科技有限公司 | Double-effect MVR forced countercurrent circulation falling film evaporation crystallization system |
Also Published As
Publication number | Publication date |
---|---|
ES2937970T3 (en) | 2023-04-03 |
EP3785782A1 (en) | 2021-03-03 |
AU2020223741A1 (en) | 2021-03-18 |
IT201900015291A1 (en) | 2021-03-02 |
US11752446B2 (en) | 2023-09-12 |
EP3785782B1 (en) | 2022-11-09 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US11377414B2 (en) | Plant and process for concentrating tartaric acid | |
US11752446B2 (en) | Plant and process for concentrating tartaric acid | |
Morison et al. | Evaporation and freeze concentration | |
US20040208967A1 (en) | Method and a system for converting liquid products into free-flowing powders with pre-cooling | |
CN110467166A (en) | A kind of wet defluorination of phosphoric acid method | |
CN105037140A (en) | Anhydrous sodium citrate production method | |
CN204034293U (en) | Lactic acid enrichment facility | |
CN103265072B (en) | A kind of basic zirconium chloride method for crystallising | |
CN202406949U (en) | Equipment for automatically producing milk powder | |
CN206198737U (en) | A kind of Acetone Retrieving Unit in isotretinoin production technology | |
CN106831321A (en) | Oxalic acid borneol acetate continuous saponification process stripping obtains the method and device of crude product borneol | |
CN204246853U (en) | A kind of cryogenic vacuum concentrator | |
CN208660399U (en) | A kind of rectifier unit for chemical industry processing | |
CN107098808B (en) | Preparation method and production device of high-purity high-content normal-temperature non-crystallized lactic acid products | |
CN105315149A (en) | Method for preparing sodium citrate | |
CN216573122U (en) | Production equipment for melting and converting ammonium thiocyanate into thiourea | |
CN110389151B (en) | Intelligent metering device for condensate condensation rate of traditional Chinese medicine concentration equipment | |
Saravacos et al. | Concentration of liquid foods in a pilot-scale falling film evaporator | |
CN215560175U (en) | Movable liquid medium and small distiller | |
CN108558642A (en) | A kind of production method of one sodium of anhydrous citric acid | |
CN104292104A (en) | Method and device for preparing methyl fluoroacetate | |
CN110433514A (en) | Double-effect falling film evaporator | |
CN117842951A (en) | Neutralization method for breaking water balance limit of mother solution | |
CN106698493A (en) | Evaporative crystallization technology of barium chloride | |
CN107986963B (en) | Process for continuously producing cyanoacetate and malonate |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
FEPP | Fee payment procedure |
Free format text: ENTITY STATUS SET TO UNDISCOUNTED (ORIGINAL EVENT CODE: BIG.); ENTITY STATUS OF PATENT OWNER: SMALL ENTITY |
|
AS | Assignment |
Owner name: DISTILLERIE MAZZARI S.P.A., ITALY Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:MARGHERITINI, EMIDIO;REEL/FRAME:053698/0542 Effective date: 20200831 |
|
FEPP | Fee payment procedure |
Free format text: ENTITY STATUS SET TO SMALL (ORIGINAL EVENT CODE: SMAL); ENTITY STATUS OF PATENT OWNER: SMALL ENTITY |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: APPLICATION DISPATCHED FROM PREEXAM, NOT YET DOCKETED |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: DOCKETED NEW CASE - READY FOR EXAMINATION |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: NON FINAL ACTION MAILED |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: RESPONSE TO NON-FINAL OFFICE ACTION ENTERED AND FORWARDED TO EXAMINER |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: NON FINAL ACTION MAILED |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: RESPONSE TO NON-FINAL OFFICE ACTION ENTERED AND FORWARDED TO EXAMINER |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: FINAL REJECTION MAILED |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: ADVISORY ACTION MAILED |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: DOCKETED NEW CASE - READY FOR EXAMINATION |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: FINAL REJECTION MAILED |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: ADVISORY ACTION MAILED |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: NON FINAL ACTION MAILED |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: RESPONSE TO NON-FINAL OFFICE ACTION ENTERED AND FORWARDED TO EXAMINER |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: NOTICE OF ALLOWANCE MAILED -- APPLICATION RECEIVED IN OFFICE OF PUBLICATIONS |
|
STPP | Information on status: patent application and granting procedure in general |
Free format text: PUBLICATIONS -- ISSUE FEE PAYMENT VERIFIED |
|
STCF | Information on status: patent grant |
Free format text: PATENTED CASE |